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中国 发明授权 有效

一种双极脉冲磁控溅射方法 【EN】Bipolar pulse magnetron sputtering method

申请(专利)号:CN201811025899.7国省代码:北京 11
申请(专利权)人:【中文】北京航空航天大学【EN】BEIHANG University
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摘要:
【中文】本发明公开一种双极脉冲磁控溅射方法,包括:一、将试样置于真空室内的样品台上,连接相关磁控溅射镀膜设备;二、完成对真空室的抽真空;三、设置双极脉冲磁控溅射电源的参数;四、向真空室内通入工作气体,通过双极脉冲磁控溅射电源施加双极脉冲电压,进行溅射沉积,完成涂层制备。本发明的优点:本发明方法可在单一靶材上实现双极脉冲磁控溅射技术,在初始负脉冲结束后施加正脉冲,驱使负脉冲产生的离子飞离靶表面附近区域,提高离子产出效率,并能够消除靶表面的电荷积累,抑制靶的打火。 【EN】The invention discloses a bipolar pulse magnetron sputtering method, which comprises the following steps: firstly, placing a sample on a sample table in a vacuum chamber, and connecting the sample with related magnetron sputtering coating equipment; secondly, vacuum pumping of the vacuum chamber is completed; thirdly, setting parameters of a bipolar pulse magnetron sputtering power supply; and fourthly, introducing working gas into the vacuum chamber, applying bipolar pulse voltage through a bipolar pulse magnetron sputtering power supply, and performing sputtering deposition to finish the preparation of the coating. The invention has the advantages that: the method can realize bipolar pulse magnetron sputtering technology on a single target, and applies positive pulse after the initial negative pulse is finished to drive ions generated by the negative pulse to fly away from the area near the target surface, thereby improving the ion output efficiency, eliminating the charge accumulation on the target surface and inhibiting the target from sparking.

主权项:
【中文】1.一种双极脉冲磁控溅射方法,其特征在于双极脉冲磁控溅射方法,包括以下步骤: 步骤一:将清洗干净的试样置于真空室内的样品台上,将双极脉冲磁控溅射电源阴极连接磁控靶,阳极接地; 步骤二:将真空腔室密封,并对真空室抽真空,待真空室的本底真空低于10Pa,完成对真空室的抽真空; 步骤三:设置双极磁控溅射电源的负脉冲的脉宽、频率以及电压,设置双极磁控溅射电源的正脉冲的脉宽、频率以及电压,设置双极磁控溅射电源的正负脉冲的频率相同而正负脉冲的脉宽可以相同也可不同,设置双极磁控溅射电源的正脉冲在负脉冲结束后产生,并设置正负脉冲的时间间隔,所述正脉冲既可施加在磁控靶上,也可施加在靶前的阳极罩或网栅上; 步骤四:向真空室内通入工作气体,设置溅射的工作气压,开启双极脉冲磁控溅射电源施加双极脉冲电压,进行溅射沉积,完成涂层制备。 【EN】1. A bipolar pulse magnetron sputtering method is characterized by comprising the following steps: the method comprises the following steps: placing the cleaned sample on a sample table in a vacuum chamber, connecting a cathode of a bipolar pulse magnetron sputtering power supply with a magnetron target, and grounding an anode; step two: sealing the vacuum chamber, and vacuumizing the vacuum chamber until the background vacuum of the vacuum chamber is lower than 10Pa, finishing the vacuum pumping of the vacuum chamber; step three: setting the pulse width, frequency and voltage of a negative pulse of a bipolar magnetron sputtering power supply, setting the pulse width, frequency and voltage of a positive pulse of the bipolar magnetron sputtering power supply, setting the frequency of the positive pulse and the frequency of the negative pulse of the bipolar magnetron sputtering power supply to be the same, setting the pulse width of the positive pulse and the pulse width of the negative pulse to be the same or different, setting the time interval of the positive pulse and the negative pulse after the negative pulse is finished, and applying the positive pulse to a magnetron target or an anode cover or a grid in front of the target; step four: and introducing working gas into the vacuum chamber, setting the sputtering working air pressure, starting a bipolar pulse magnetron sputtering power supply to apply bipolar pulse voltage, and performing sputtering deposition to finish the preparation of the coating.


说明书

【中文】

一种双极脉冲磁控溅射方法

技术领域

本发明涉及材料表面工程,尤其涉及脉冲磁控溅射。

背景技术

磁控溅射技术以其低温沉积、表面光滑、无颗粒缺陷等诸多优点广泛应用于薄膜制备领域,但传统的磁控溅射处理技术溅射金属大多以原子状态存在,金属离化率低(~1%),导致其可控性较差,沉积薄膜的质量和性能较难优化。针对该问题,国外学者开发出了一种高功率脉冲磁控溅射技术,其在放电过程中的峰值功率可超过普通磁控溅射2个数量级,达10kw/cm2,靶周围的电子密度可达1019/m3,同时溅射材料的离化率最高可达90%以上,使得该技术在溅射领域引起了极大关注,并在拓展各种应用。

然而,高功率脉冲磁控溅射需要较高的负电压来实现磁控放电,这会使溅射出来的靶材原子离化成离子后又被靶的负电压给吸引回来。这种被吸引回来的靶材离子一方面参与自溅射过程,另一个方面由于被吸引回来而不能到达工件表面,导致高功率脉冲磁控溅射的沉积效率不高。此外,在反应溅射过程中,由于磁控靶同样与反应气体发生反应而形成化合物,导致靶表面打火,影响高功率脉冲磁控溅射技术制备化合物薄膜的稳定性。

发明内容

本发明之目的是针对现有高功率脉冲磁控溅射技术的不足和缺陷,提供一种双极脉冲磁控溅射方法,以提高高功率脉冲磁控溅射的沉积效率及其在制备化合物薄膜中的稳定性。

为实现上述目的,本发明提供一种双极脉冲磁控溅射方法,包括:

步骤一:将清洗干净的试样置于真空室内的样品台上,将双极脉冲磁控溅射电源阴极连接磁控靶,阳极接地;

步骤二:将真空腔室密封,并对真空室抽真空,待真空室的本底真空低于10-2Pa,完成对真空室的抽真空;

步骤三:设置双极磁控溅射电源的负脉冲的脉宽、频率以及电压,设置双极磁控溅射电源的正脉冲的脉宽、频率以及电压,设置双极磁控溅射电源的正负脉冲的频率相同而正负脉冲的脉宽可以相同也可不同,设置双极磁控溅射电源的正脉冲在负脉冲结束后产生,并设置正负脉冲的时间间隔。

步骤四:向真空室内通入工作气体,设置溅射的工作气压,开启双极脉冲磁控溅射电源施加双极脉冲电压,进行溅射沉积,完成涂层制备。

作为优选方式,所述正脉冲在负脉冲结束后施加,正负脉冲的时间间隔为0μs~500μs。

作为优选方式,所述正脉冲既可施加在磁控靶上,也可施加在靶前的阳极罩或网栅上。

作为优选方式,所述阳极罩可为平板也可为桶状或锥状;所述桶状或锥状阳极罩的内壁轮廓为圆形、椭圆形或多边形。

作为优选方式,所述网栅的形状可为圆形、椭圆形或多边形。

作为优选方式,所述双极磁控溅射电源的负脉冲为高功率脉冲,负脉冲的电压为200V~2000V。

作为优选方式,所述双极磁控溅射电源的负脉冲的脉宽为3μs~1ms。

作为优选方式,所述双极磁控溅射电源的正脉冲的电压为1V~2000V。

作为优选方式,所述双极磁控溅射电源的正脉冲的脉宽为3μs~1ms。

作为优选方式,所述双极磁控溅射电源的正负脉冲的频率为5Hz~100kHz。

作为优选方式,所述工作气体可以为惰性气体或反应气体的一种或几种气体的混合气体。

作为优选方式,所述工作气压为0Pa~50Pa。

本发明应用于材料表面工程领域。

本发明的优点:本发明方法可在单靶材上实现双极脉冲磁控溅射技术,在初始负脉冲结束后施加正脉冲,正脉冲既可施加在磁控靶上也可施加在靶前的阳极罩或网栅上,正脉冲可驱使由负脉冲在靶表面附近区域产生的离子飞离靶所在区域,避免将溅射出来的靶材原子离化成离子后,又被吸回到靶材,提高沉积效率,并能够消除靶表面的电荷积累,抑制靶的打火,提高离子能量。

附图说明

为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅用于解释本发明的构思。

图1为本发明的双极脉冲磁控溅射的正脉冲施加到磁控靶的设备装置示意图。

图2为本发明的双极脉冲磁控溅射的正脉冲施加到磁控靶前的阳极罩或网栅的设备装置示意图。

图3是试验一的实际电压与电流波形图。

图4是试验二的实际电压与电流波形图。

图5是试验三的实际电压与电流波形图。

附图标记汇总:

1、反应气体 2、真空室 3、试样

4、样品台 5、抽真空系统 6、磁控靶

7、双极脉冲磁控溅射电源 8、阳极罩 9、网栅

10、切换开关

具体实施方式

在下文中,将参照附图描述本发明的一种双极脉冲磁控溅射方法的实施例。

在此记载的实施例为本发明的特定的具体实施方式,用于说明本发明的构思,均是解释性和示例性的,不应解释为对本发明实施方式及本发明范围的限制。除在此记载的实施例外,本领域技术人员还能够基于本申请权利要求书和说明书所公开的内容采用显而易见的其它技术方案,这些技术方案包括对在此记载的实施例做出任何显而易见的替换和修改的技术方案。

本说明书的附图为示意图,辅助说明本发明的构思,示意性地表示各部分的形状及其相互关系。请注意,为了便于清楚地表现出本发明实施例的各部分的结构,各附图之间不一定按照相同的比例绘制。相同或相似的参考标记用于表示相同或相似的部分。

图1为本发明的双极脉冲磁控溅射的正脉冲施加到磁控靶的设备装置示意图。如图1所示,在本实施例中,本发明提供一种双极脉冲磁控溅射方法,包括工作气体1、真空室2、试样3、样品台4、抽真空系统5、磁控靶6以及双极脉冲磁控溅射电源7。

图2为本发明的双极脉冲磁控溅射的正脉冲施加到磁控靶前的阳极罩8或网栅9的设备装置示意图。该装置在磁控靶6前安装阳极罩8或网栅9,其中正脉冲施加在阳极罩8或网栅9上由切换开关10控制。其它结构与图1相同。

示例1:本实施方案是通过选择高纯钛靶作为磁控靶6,氩气和氮气作为工作气体1,采用双极磁控溅射技术在单晶硅表面制备TiN薄膜,采取图1中的装置。

具体步骤如下:

步骤(1):将清洗干净的试样3置于真空室2内的样品台4上,将双极脉冲磁控溅射电源7阴极连接高纯磁控钛靶6,阳极接地;

步骤(2):将真空室2密封,并对真空室2抽真空,待真空室2的本底真空低于10-2Pa,完成对真空室2的抽真空;

步骤(3):设置双极磁控溅射电源7的负脉冲的脉宽为3μs~1ms、频率为5Hz~100kHz以及电压为200V~2000V,设置双极磁控溅射电源7的正脉冲的3μs~1ms和频率为5Hz~100kHz,正脉冲电压分别设置为0V,50V,100V,设置双极磁控溅射电源7的正负脉冲的频率相同,设置双极磁控溅射电源7的正脉冲在负脉冲结束后产生,并设置正负脉冲的时间间隔为0μs。

步骤(4):向真空室2内通入工作气体1(氩气和氮气),设置溅射的工作气压0.1Pa~5Pa,开启双极脉冲磁控溅射电源7给磁控靶6施加双极脉冲电压,进行溅射沉积,溅射时间为1min~1000min,完成TiN涂层的制备。

图3是试验一正脉冲电压不同的实际电压与电流波形图。从图中可以看出高纯钛靶的靶电压分别具有负脉冲和正脉冲,并且在初始负脉冲结束之后立既施加了正脉冲,说明本试验实现了单一靶材的双极脉冲磁控溅射方法,且正脉冲的电压可调。

示例2:本实施例与示例1的不同点是:设置双极磁控溅射电源7的正脉冲的脉宽分别为100μs和200μs,其它步骤与示例1相同。

图4是试验二正脉冲脉宽不同的实际电压与电流波形图。从图中可以看出本试验实现了单一靶材的双极脉冲磁控溅射方法,且正脉冲的脉宽可调。

示例3:本实施例与示例1的不同点是:设置双极磁控溅射电源7的正负脉冲时间间隔分别为0μs和20μs,其它步骤与示例1相同。

图5是试验三正负脉冲时间间隔不同的实际电压与电流波形图。从图中可以看出本试验实现了单一靶材的双极脉冲磁控溅射方法,且在初试负脉冲结束后可立既施加正脉冲,也可在一定时间间隔后施加正脉冲。

示例4:本实施方案是通过选择高纯钛靶作为磁控靶6,氩气和氧气作为工作气体1,采用双极磁控溅射技术在单晶硅表面制备TiO2薄膜,采取图1中的装置。本实施例与第一实施例的不同点是:氩气和氧气作为工作气体1,其它步骤与示例1相同。

示例5:本实施方案是通过选择高纯铝靶作为磁控靶,氩气和氧气作为工作气体1,采用双极磁控溅射技术在单晶硅表面制备Al2O3薄膜,采取图1中的装置。本实施例与示例4的不同点是:磁控靶6为高纯铝靶,其它步骤与示例4相同。

示例6:本实施方案是通过选择高纯钛靶作为磁控靶6,氩气和氮气作为工作气体1,采用双极磁控溅射技术在单晶硅表面制备TiN薄膜,采取图2的装置。本实施例与示例1不同点是:采用的设备装置为图2装置,正脉冲施加在磁控靶6前的阳极罩8或网栅9上,其中正脉冲施加在阳极罩8或网栅9上由切换开关10控制,其它步骤与示例1相同。

以上对本发明的双极脉冲磁控溅射方法及其操作方法的实施方式进行了说明,其目的在于解释本发明之精神。对于本发明的双极脉冲磁控溅射方法的具体特征如双极脉冲时间间隔和正脉冲开始施加方式可以根据上述披露的特征的作用进行具体设计,这些设计均是本领域技术人员能够实现的。而且,上述披露的各技术特征并不限于已披露的与其它特征的组合,本领域技术人员还可根据本发明之目的进行各技术特征之间的其它组合,以实现本发明之目的为准。

【EN】

Bipolar pulse magnetron sputtering method

Technical Field

The invention relates to material surface engineering, in particular to pulse magnetron sputtering.

Background

The magnetron sputtering technology is widely applied to the field of film preparation by virtue of the advantages of low-temperature deposition, smooth surface, no particle defect and the like, but the traditional magnetron sputtering treatment technology has the defects that most of sputtered metal exists in an atomic state and the ionization rate of the metal is low (1 percent), so that the controllability is poor, and the quality and the performance of a deposited film are difficult to optimize. Aiming at the problem, foreign scholars develop a high-power pulse magnetron sputtering technology, the peak power of the high-power pulse magnetron sputtering technology can exceed 2 orders of magnitude of that of common magnetron sputtering in the discharge process and reaches 10kw/cm2Electron density around the target of up to 1019/m3Meanwhile, the ionization rate of the sputtering material can reach more than 90 percent, so that the technology draws great attention in the sputtering field and expands various applications.

However, high power pulsed magnetron sputtering requires a high negative voltage to achieve magnetron discharge, which causes sputtered target material atoms to be ionized into ions and then attracted back by the negative voltage of the target. The attracted target ions participate in the self-sputtering process on one hand, and cannot reach the surface of the workpiece on the other hand due to being attracted back, so that the deposition efficiency of the high-power pulse magnetron sputtering is not high. In addition, in the reactive sputtering process, the magnetron target also reacts with the reaction gas to form a compound, so that the surface of the target is ignited, and the stability of the compound film prepared by the high-power pulse magnetron sputtering technology is influenced.

Disclosure of Invention

The invention aims to provide a bipolar pulse magnetron sputtering method aiming at the defects of the existing high-power pulse magnetron sputtering technology so as to improve the deposition efficiency of high-power pulse magnetron sputtering and the stability of the high-power pulse magnetron sputtering in preparing a compound film.

In order to achieve the above object, the present invention provides a bipolar pulse magnetron sputtering method, comprising:

the method comprises the following steps: placing the cleaned sample on a sample table in a vacuum chamber, connecting a cathode of a bipolar pulse magnetron sputtering power supply with a magnetron target, and grounding an anode;

step two: sealing the vacuum chamber, and vacuumizing the vacuum chamber until the background vacuum of the vacuum chamber is lower than 10-2Pa, finishing the vacuum pumping of the vacuum chamber;

step three: the pulse width, the frequency and the voltage of a negative pulse of the bipolar magnetron sputtering power supply are set, the pulse width, the frequency and the voltage of a positive pulse of the bipolar magnetron sputtering power supply are set, the frequency of the positive pulse and the frequency of the negative pulse of the bipolar magnetron sputtering power supply are the same, the pulse width of the positive pulse and the pulse width of the negative pulse can be the same or different, the positive pulse of the bipolar magnetron sputtering power supply is generated after the negative pulse is finished, and the time interval of the positive pulse and the negative pulse is set.

Step four: and introducing working gas into the vacuum chamber, setting the sputtering working air pressure, starting a bipolar pulse magnetron sputtering power supply to apply bipolar pulse voltage, and performing sputtering deposition to finish the preparation of the coating.

Preferably, the positive pulse is applied after the negative pulse is ended, and the time interval between the positive pulse and the negative pulse is 0 μ s to 500 μ s.

Preferably, the positive pulse is applied to either the magnetron target or the anode shield or mesh grid in front of the target.

Preferably, the anode cover can be a flat plate, a barrel shape or a cone shape; the inner wall of the barrel-shaped or cone-shaped anode cover is circular, oval or polygonal in outline.

Preferably, the shape of the mesh can be circular, elliptical or polygonal.

Preferably, the negative pulse of the bipolar magnetron sputtering power supply is a high-power pulse, and the voltage of the negative pulse is 200V-2000V.

Preferably, the pulse width of the negative pulse of the bipolar magnetron sputtering power supply is 3 μ s to 1 ms.

Preferably, the positive pulse voltage of the bipolar magnetron sputtering power supply is 1V to 2000V.

Preferably, the pulse width of the positive pulse of the bipolar magnetron sputtering power supply is 3 μ s to 1 ms.

Preferably, the frequency of the positive and negative pulses of the bipolar magnetron sputtering power supply is 5Hz to 100 kHz.

Preferably, the working gas may be one or a mixture of several of inert gases or reactive gases.

Preferably, the working gas pressure is 0 to 50 Pa.

The invention is applied to the field of material surface engineering.

The invention has the advantages that: the method can realize bipolar pulse magnetron sputtering technology on a single target material, and applies positive pulse after the initial negative pulse is finished, wherein the positive pulse can be applied to a magnetron target and an anode cover or a grid in front of the target, and can drive ions generated by the negative pulse in the area near the target surface to fly away from the area where the target is located, so that the sputtered target material atoms are prevented from being absorbed back to the target material after being ionized into ions, the deposition efficiency is improved, the charge accumulation on the target surface can be eliminated, the target is inhibited from being ignited, and the ion energy is improved.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only used for explaining the concept of the present invention.

FIG. 1 is a schematic diagram of an apparatus for applying positive pulses to a magnetron target in bipolar pulse magnetron sputtering according to the present invention.

FIG. 2 is a schematic diagram of the apparatus of the anode shield or mesh grid before the positive pulse is applied to the magnetron target in the bipolar pulse magnetron sputtering of the present invention.

Fig. 3 is a graph of the actual voltage and current waveforms of test one.

Fig. 4 is a graph of the actual voltage and current waveforms for test two.

Fig. 5 is a graph of the actual voltage and current waveforms for test three.

Summary of reference numerals:

1. reaction gas 2, vacuum chamber 3, sample

4. Sample stage 5, vacuum pumping system 6, magnetic control target

7. Bipolar pulse magnetron sputtering power supply 8, anode cover 9 and mesh grid

10. Change-over switch

Detailed Description

Hereinafter, an embodiment of a bipolar pulse magnetron sputtering method of the present invention will be described with reference to the drawings.

The examples described herein are specific embodiments of the present invention, are intended to be illustrative and exemplary in nature, and are not to be construed as limiting the scope of the invention. In addition to the embodiments described herein, those skilled in the art will be able to employ other technical solutions which are obvious based on the disclosure of the claims and the specification of the present application, and these technical solutions include any obvious replacement or modification of the embodiments described herein.

The drawings in the present specification are schematic views to assist in explaining the concept of the present invention, and schematically show the shapes of respective portions and their mutual relationships. It is noted that the drawings are not necessarily to the same scale so as to clearly illustrate the structure of portions of embodiments of the present invention. The same or similar reference numerals are used to denote the same or similar parts.

FIG. 1 is a schematic diagram of an apparatus for applying positive pulses to a magnetron target in bipolar pulse magnetron sputtering according to the present invention. As shown in fig. 1, in the present embodiment, the present invention provides a bipolar pulse magnetron sputtering method, which includes a working gas 1, a vacuum chamber 2, a sample 3, a sample stage 4, a vacuum pumping system 5, a magnetron target 6, and a bipolar pulse magnetron sputtering power supply 7.

Fig. 2 is a schematic diagram of the device arrangement of the anode cover 8 or the mesh 9 before the positive pulse of the bipolar pulse magnetron sputtering is applied to the magnetron target. The device is provided with an anode cover 8 or a mesh grid 9 in front of a magnetron target 6, wherein positive pulses are applied to the anode cover 8 or the mesh grid 9 and are controlled by a selector switch 10. The other structure is the same as that of fig. 1.

Example 1: in the embodiment, a high-purity titanium target is selected as a magnetron target 6, argon and nitrogen are used as working gas 1, a TiN film is prepared on the surface of monocrystalline silicon by adopting a bipolar magnetron sputtering technology, and the device in the figure 1 is adopted.

The method comprises the following specific steps:

step (1): placing a cleaned sample 3 on a sample table 4 in a vacuum chamber 2, connecting a cathode of a bipolar pulse magnetron sputtering power supply 7 with a high-purity magnetron titanium target 6, and grounding an anode;

step (2): sealing the vacuum chamber 2, and vacuumizing the vacuum chamber 2 until the background vacuum of the vacuum chamber 2 is lower than 10-2Pa, finishing the vacuum pumping of the vacuum chamber 2;

and (3): setting the pulse width of a negative pulse of a bipolar magnetron sputtering power supply 7 to be 3 mus-1 ms, the frequency to be 5 Hz-100 kHz and the voltage to be 200V-2000V, setting the 3 mus-1 ms and the frequency of a positive pulse of the bipolar magnetron sputtering power supply 7 to be 5 Hz-100 kHz, setting the positive pulse voltage to be 0V, 50V and 100V respectively, setting the frequency of a positive pulse and a negative pulse of the bipolar magnetron sputtering power supply 7 to be the same, setting the positive pulse of the bipolar magnetron sputtering power supply 7 to be generated after the negative pulse is finished, and setting the time interval of the positive pulse and the negative pulse to be 0 mus.

And (4): and (3) introducing working gas 1 (argon and nitrogen) into the vacuum chamber 2, setting the sputtering working pressure to be 0.1-5 Pa, starting a bipolar pulse magnetron sputtering power supply 7 to apply bipolar pulse voltage to a magnetron target 6, and performing sputtering deposition for 1-1000 min to finish the preparation of the TiN coating.

FIG. 3 is a graph of actual voltage and current waveforms for testing a positive pulse voltage for various reasons. The target voltage of the high-purity titanium target is respectively provided with a negative pulse and a positive pulse, and the positive pulse is applied immediately after the initial negative pulse is finished, so that the test realizes the bipolar pulse magnetron sputtering method of the single target, and the voltage of the positive pulse is adjustable.

Example 2: the present embodiment is different from example 1 in that: the pulse widths of the positive pulses of the bipolar magnetron sputtering power supply 7 were set to 100 μ s and 200 μ s, respectively, and the other steps were the same as in example 1.

Fig. 4 is a graph of actual voltage and current waveforms for testing the pulse widths of two positive pulses. It can be seen from the figure that the test realizes the bipolar pulse magnetron sputtering method of the single target material, and the pulse width of the positive pulse is adjustable.

Example 3: the present embodiment is different from example 1 in that: the positive and negative pulse time intervals of the bipolar magnetron sputtering power source 7 were set to 0 μ s and 20 μ s, respectively, and the other steps were the same as in example 1.

Fig. 5 is a graph of actual voltage and current waveforms for three different time intervals of positive and negative pulses tested. It can be seen from the figure that the test realizes the bipolar pulse magnetron sputtering method of the single target, and the positive pulse can be applied immediately after the initial negative pulse is finished, or the positive pulse can be applied after a certain time interval.

Example 4: the embodiment adopts the bipolar magnetron sputtering technology to prepare TiO on the surface of monocrystalline silicon by selecting a high-purity titanium target as a magnetron target 6 and argon and oxygen as working gases 12The film was the device of FIG. 1. The present embodiment is different from the first embodiment in that: argon and oxygen were used as the working gas 1, and the other steps were the same as in example 1.

Example 5: the embodiment adopts the bipolar magnetron sputtering technology to prepare Al on the surface of the monocrystalline silicon by selecting a high-purity aluminum target as a magnetron target and argon and oxygen as working gases 12O3The film was the device of FIG. 1. The present embodiment is different from example 4 in that: the magnetron target 6 was a high purity aluminum target, and the other steps were the same as in example 4.

Example 6: according to the embodiment, a high-purity titanium target is selected as a magnetron target 6, argon and nitrogen are used as working gas 1, a TiN film is prepared on the surface of monocrystalline silicon by adopting a bipolar magnetron sputtering technology, and the device shown in figure 2 is adopted. The present embodiment differs from example 1 in that: the device adopted is the device shown in FIG. 2, positive pulses are applied to the anode cover 8 or the mesh grid 9 in front of the magnetron target 6, wherein the positive pulses are applied to the anode cover 8 or the mesh grid 9 and controlled by a change-over switch 10, and other steps are the same as those of the example 1.

The embodiments of the bipolar pulse magnetron sputtering method and the operation method thereof according to the present invention are explained above, and the purpose thereof is to explain the spirit of the present invention. The specific features of the bipolar pulsed magnetron sputtering method of the present invention, such as the bipolar pulse time interval and the positive pulse initiation application pattern, can be specifically designed in accordance with the effects of the features disclosed above, and such designs are within the reach of those skilled in the art. Moreover, the technical features disclosed above are not limited to the combinations with other features disclosed, and other combinations between the technical features can be performed by those skilled in the art according to the purpose of the present invention, so as to achieve the purpose of the present invention.

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